Gramine recrystallization

[dmtmd]

What is a good recrystallizing solvent to separate dmt from gramine. For any solvent to meet these requirements it must be so that gramine is soluble in it at all temperatures but dmt is only soluble in it at higher temperatures.

Also i would like it if someone can confirm that hordenine can be romoved from dmt by vacuum distillation.

Thanks in advanced.

 

[endlessness]

This has been discussed before, check the FAQ, the phalaris link in my signature. Hexane, heptane or normal aliphatic naphtha are good solvents to separate gramine and hordenine from dmt. Cold limonene works decently too, but better repeat at least once.

The title is a bit misleading, seems you want gramine ? FASA works good for recrystallizing gramine according to tests I made but not to separate DMT, so you if you want gramine for some reason (like for example as ref standard for TLC), then after you pull your dmt/gramine mixture with naphtha, pull with a less selective solvent like xylene or so, which should pull your gramine, and then do FASA on it to precipitate gramine needles.

 

[dmtmd]

Sorry for the misleading title, my intention is to recrystallize dmt and to discard the gramine in the room temp solvent. When you say repeat once with a lemonine pull are you referring to salting the dmt then rebasing then re pulling with more lemonine? I would also like to note pulling with a solvent like naptha that only the dmt is soluble in is not recrystallization. And when you refer to using xylene with naptha to separate gramine, are you talking about mixing the naptha solution with xylene in a seperatory funnel and shaking then separating.

 

[endlessness]

Yes regarding the repeat limonene pull

As for pulling with naphtha, it is recrystallization if you already have gotten some crystals (or crude product) some other way such as xylene pulls, and then do the naphtha pull afterwards.

What I said about xylene on last post is to first pull with naphtha, then after having separated the naphtha pull, use xylene on your basic soup, or you can do the inverse, first pull with xylene to get everything, then use naphtha just on the crude product resulting from your xylene salting/freebasing or evaporating.

 

[dmtmd]

Wouldnt the purpose of xylene be to only dissolve the gramine and not the dmt? In that case how would you do the initial pull with xylene and end up with dmt in said solvent? Or are you saying use xylene to remove gramine from plant material then basify the plant material and pull with naptha?

 

[endlessness]

No, xylene dissolves both dmt and gramine (possibly hordenine too but I dont know since I never had access to pure hordenine). So you can use xylene first to get both alkaloids, then naphtha to get just dmt, or you use naphtha to get just dmt, then xylene to get other alkaloids that are left behind after you got most DMT out, if you want other alkaloids for some reason. If you just want DMT, go for just naphtha. Just make sure your naphtha is purely aliphatic hydrocarbons and doesnt contain aromatic ones (like mixed in xylene, toluene etc)